Hot Hydrogen Testing of Refractory Metals and Ceramics

The objective of this investigation is to develop a technique with which refractory metal carbide samples can be exposed to hydrogen containing gases at high temperatures, and to use various microstructural and analytical techniques to determine the chemical and rate processes involved in hydrogen degradation in these materials. Five types of carbides were examined including WC, NbC, HfC, ZrC, and TaC. The ceramics were purchased and were all monolithic in nature. The temperature range investigated was from 850 to 1600 C with a hydrogen pressure of one atmosphere. Control experiments, in vacuum, were also conducted for comparison so that the net effects due to hydrogen could be isolated. The samples were analyzed prior to and after exposure. Gas samples were collected in selected experiments and analyzed using gas chromography. Characterization of the resulting microstructure after exposure to hydrogen was conducted using optical microscopy, x-ray diffraction, scanning electron microscopy, and weight change. The ceramics were purchased and were all monolithic in nature. It was found that all samples lost weight after exposure, both in hydrogen and vacuum. Results from the microstructure analyses show that the degradation processes are different among the five types of ceramics involved. In addition, the apparent activation energy for the degradation process is a function of temperature even within the same material. This indicates that there are more than one mechanism involved in each material, and that the mechanisms are temperature dependent.